CN113667417B - Electromagnetic wave radiation preventing optical adhesive and preparation method thereof - Google Patents
Electromagnetic wave radiation preventing optical adhesive and preparation method thereof Download PDFInfo
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- CN113667417B CN113667417B CN202111020793.XA CN202111020793A CN113667417B CN 113667417 B CN113667417 B CN 113667417B CN 202111020793 A CN202111020793 A CN 202111020793A CN 113667417 B CN113667417 B CN 113667417B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
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Abstract
The invention belongs to the technical field of optical cement, and provides an optical cement for preventing electromagnetic wave radiation and a preparation method thereof aiming at the problems that the electromagnetic wave radiation prevention performance of the optical cement is weak and the combination of nano materials and the optical cement is not firm40Fe40B20The acrylic adhesive is obtained by alternately laying acrylic adhesive compounded with graphene and respectively attaching heavy release films and light release films to the two surfaces of the acrylic adhesive, wherein Co is compounded40Fe40B20The acrylate adhesive and the acrylate adhesive compounded with graphene have the same number of layers, and Co is compounded in one-step laying40Fe40B20The acrylate adhesive and the acrylate adhesive compounded with graphene at one time are used as one layer, the number of the paving layers is 3-5, the phenomenon that nano particles are agglomerated and the stability of the combination of the nano particles and the adhesive is not strong is avoided, the mechanical property of the optical adhesive is improved, the process of absorption-reflection-reabsorption can be formed in the optical adhesive, and the efficient electromagnetic radiation wave effect is realized.
Description
Technical Field
The invention belongs to the technical field of optical cement, and particularly relates to electromagnetic wave radiation prevention optical cement and a preparation method thereof.
Background
With the rapid development of the electronic information industry, electromagnetic pollution is increasingly serious, and electromagnetic interference can be caused to electronic equipment. Modern medicine has demonstrated that long-term electromagnetic radiation can affect the health of the human body. Electromagnetic interference shielding materials are of great interest because of their critical role in blocking unwanted electromagnetic radiation. Many materials, including metals, carbon materials, and metal oxides, have been extensively studied in this field.
The existing optical adhesive film has single function and weak electromagnetic wave radiation resistance. The conductive filler endows the optical cement with electromagnetic shielding capability, and common electromagnetic shielding materials are electromagnetic shielding materials containing metal layer interlayers or doped metal particles, but the combination of the metal or nano materials and the optical cement is not firm, and the metal or nano materials are not uniformly dispersed in the optical cement, so that the absorption or reflection of electromagnetic waves is incomplete, secondary electromagnetic radiation pollution is easily caused, the use and protection performance of the optical cement is poor, and the requirements of users are difficult to meet.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an anti-electromagnetic radiation optical cement which is compounded with Co40Fe40B20The acrylic adhesive is obtained by alternately laying acrylic adhesive compounded with graphene and respectively attaching heavy release films and light release films to the two surfaces of the acrylic adhesive, wherein Co is compounded40Fe40B20The laying number of the acrylate adhesive compounded with the graphene is the same, and Co is compounded in one laying40Fe40B20The acrylic adhesive and the acrylic adhesive compounded with graphene at one time are used as one layer, and the number of the laying layers is 3-5.
Preferably, the heavy release film and the light release film are both ultra-light fluorine release films, the release force of the heavy release film is 25-35g, and the release force of the light release film is 8-14 g.
In order to achieve the purpose, the invention is realized by the following scheme:
a preparation method of an electromagnetic wave radiation preventing optical cement comprises the following steps:
(1) adding graphene oxide into deionized water, carrying out ultrasonic treatment for 2h, dispersing uniformly to obtain a suspension, and adding NaOH and ClCH under continuous stirring2COOH，After the dripping is finished, carrying out ultrasonic treatment again, carrying out water dialysis treatment on the mixture, then carrying out hot filtration on the dispersion liquid by using filter paper, collecting filtrate after a large number of graphene sheets pass through the filter paper, evaporating the solvent by using a rotary evaporator, and drying to obtain carboxylated graphene;
(2) mixing boron block and FeCl2·4H2O and CoCl2·6H2Dissolving O in deionized water, adding polyacrylic acid into the solution, adding precipitant, stirring to obtain black solution, growing at 80 deg.C for 30min, and drying to obtain polyacrylic acid @ Co40Fe40B20Powder;
(3) dissolving an emulsifier SE-10 in deionized water, transferring the deionized water into a constant temperature reactor, heating the deionized water to 80 ℃ under continuous stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving hydroxyethyl acrylate in the deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, and stirring for 15min for pre-emulsification to obtain an emulsion;
(4) adding 20% of the emulsion into a reactor, adding another 1 part of SE-10 solution of the emulsifier, stirring uniformly, adding ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain a seed emulsion, dividing the seed emulsion into two parts, dividing the rest of the emulsion into two parts, respectively adding the seed emulsion into the seed emulsion, and respectively adding the carboxylated graphene and the polyacrylic acid @ Co under continuous stirring40Fe40B20Respectively carrying out ultrasonic treatment reaction on the powder, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust to a target pH value, and filtering to respectively obtain the graphene-compounded acrylate adhesive and Co-compounded acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20The acrylate adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp every time, and finally the light release film is attached to the top layer to obtain the electromagnetic wave radiation resistant optical adhesive.
Preferably, the particle size of the graphene oxide in the step (1) is 10-50 nm.
Preferably, the graphene oxide, NaOH and ClCH in the step (1)2The mass ratio of COOH is 0.4-0.6:5:9-11, the ultrasonic treatment time after the dropwise addition of NaOH and ClCH2COOH in the step (1) is 3-4h, the water dialysis treatment time is 45-48h, and the drying condition is drying in an oven at 60 ℃ for 12-18 h.
Preferably, in the step (2), polyacrylic acid, boron block and FeCl are used2·4H2O、CoCl2·6H2The mass ratio of O to deionized water is 18-25:1-1.2:39-40:47-47.5:100, and the precipitator in the step (2) is 0.1M sodium hydroxide solution, and the amount of the precipitator is 1/10 of deionized water.
Preferably, the drying condition in the step (2) is drying in a vacuum oven at 50 ℃ for 24 h.
Preferably, the emulsifier SE-10 in the step (3) is SE-10, the mass ratio of the emulsifier SE-10 to hydroxyethyl acrylate is 1-3:75-85, the mass ratio of the emulsifier SE-10 to deionized water is 1-3:10-15, and the mass ratio of the hydroxyethyl acrylate to the deionized water is 75-85: 50-60.
Preferably, in the step (4), the carboxylated graphene, polyacrylic acid @ Co40Fe40B20The mass ratio of the powder to the emulsion to the ammonium persulfate is 4-5:10-15:80-86: 1-2.
Preferably, the reaction condition of the ultrasonic treatment in the step (4) is that the ultrasonic dispersion is carried out for 20min, then the reaction is carried out for 3-4h by heating to 80 ℃, and the target pH is 7-8.
Compared with the prior art, the method has the beneficial effects that:
(1) the invention provides an electromagnetic wave radiation preventing optical cement and a preparation method thereof, which are characterized in that graphene oxide and Co are respectively mixed40Fe40B20Adding the carboxylated graphene oxide into a hydroxyethyl acrylate emulsifier, and reacting carboxyl with hydroxyl to obtain graphene oxide and Co40Fe40B20Grafted to the hydroxyethyl polyacrylate respectively, on one hand, the dispersibility of the nanoparticles in the hydroxyethyl polyacrylate is improved, and on the other hand, the nanoparticles can be respectively grafted to the hydroxyethyl polyacrylateThe stable combination of the nano-particles and the colloid avoids the phenomena of nano-particle agglomeration and poor stability of the nano-particles and the colloid, and also improves the mechanical property of the optical adhesive.
(2) The invention provides an anti-electromagnetic radiation optical cement, wherein Co is compounded40Fe40B20The magnetism of the acrylate adhesive tape has high-efficiency absorption capacity on electromagnetic radiation, the acrylate adhesive compounded with the graphene has reflection capacity on the electromagnetic radiation, the acrylate adhesive tape and the graphene have synergistic effect, multiple layers are overlapped to generate an absorption-reflection-reabsorption process inside, multiple reflections and scattering are formed inside the acrylate adhesive tape, the self consumption of the electromagnetic radiation inside the film is realized, and the high-efficiency electromagnetic radiation wave shielding effect is realized.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An electromagnetic wave radiation preventing optical cement and a preparation method thereof, comprising the following steps:
(1) adding 0.4g of graphene oxide into 50ml of deionized water, carrying out ultrasonic treatment for 2h, uniformly dispersing to obtain a suspension, and adding 5g of NaOH and 9g of ClCH under continuous stirring2After the COOH is added dropwise, carrying out ultrasonic treatment for 3 hours, carrying out dialysis treatment on the mixture for 45 hours, then carrying out hot filtration on the dispersion liquid by using filter paper, collecting filtrate after a large number of graphene sheets pass through the filter paper, evaporating the solvent by using a rotary evaporator, and drying in an oven at 60 ℃ for 12 hours to obtain carboxylated graphene;
(2) 1g of boron block, 39g of FeCl2·4H2O and 47gCoCl2·6H2Dissolving O in 100ml deionized water, adding 18g polyacrylic acid into the solution, adding 10g0.1M sodium hydroxide solution, stirring to obtain black solution, growing at 80 deg.C for 30min, and vacuum oven at 50 deg.CAfter drying for 24h, the product obtained is polyacrylic acid @ Co40Fe40B20Powder;
(3) dissolving 1g of emulsifier SE-10 in 10ml of deionized water, transferring the solution to a constant temperature reactor, heating the solution to 80 ℃ and continuously stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving 75g of hydroxyethyl acrylate in 50ml of deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, stirring for 15min, and pre-emulsifying to obtain an emulsion;
(4) adding 20% of 80g of emulsion into a reactor, adding another 1 part of SE-10 solution of the emulsifier, stirring uniformly, adding 1g of ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain seed emulsion, dividing the seed emulsion into two parts, dividing the rest of the emulsion into two parts, respectively adding the seed emulsion into the seed emulsion, and respectively adding 4g of carboxylated graphene and 10g of polyacrylic acid @ Co under continuous stirring40Fe40B20Respectively ultrasonically dispersing the powder for 20min, heating to 80 ℃ for reaction for 3h, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust the pH to 7, and filtering to respectively obtain the graphene-compounded acrylate adhesive and Co-compounded acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20The acrylate adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp once, 3 layers are coated, and finally the light release film is attached to the top layer to obtain the electromagnetic wave radiation resistant optical adhesive.
Example 2
An electromagnetic wave radiation preventing optical cement and a preparation method thereof, comprising the following steps:
(1) adding 0.5g of graphene oxide into 50ml of deionized water, carrying out ultrasonic treatment for 2h, uniformly dispersing to obtain a suspension, and adding 5g of NaOH and 9.5g of ClCH under continuous stirring2COOH, the ultrasonic treatment time is 3.2h after the dripping is finished, the mixture is dialyzed against water for 46h, then the dispersion is filtered by filter paper, and a large number of graphene sheets are filtered by the filter paperAfter paper is made, collecting filtrate, evaporating the filtrate to dryness by using a rotary evaporator, and drying in an oven at 60 ℃ for 14 hours to obtain carboxylated graphene;
(2) 1.2g of boron block, 39.5g of FeCl2·4H2O and 47.2gCoCl2·6H2Dissolving O in 100ml deionized water, adding 20g of polyacrylic acid into the solution, adding 10g of 0.1M sodium hydroxide solution, stirring uniformly to form a black solution, growing at 80 ℃ for 30min, and drying in a vacuum oven at 50 ℃ for 24h to obtain a product of @ polyacrylic acid Co40Fe40B20Powder;
(3) dissolving 1.5g of emulsifier SE-10 in 10ml of deionized water, transferring the solution to a constant temperature reactor, heating the solution to 80 ℃ and continuously stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving 80g of hydroxyethyl acrylate in 50ml of deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, stirring for 15min, and pre-emulsifying to obtain an emulsion;
(4) adding 20% of 82g of emulsion into a reactor, adding another 1 part of SE-10 solution of the emulsifier, stirring uniformly, adding 1.2g of ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain a seed emulsion, dividing the seed emulsion into two parts, dividing the rest of the emulsion into two parts, respectively adding the two parts into the seed emulsion, and respectively adding 4.2g of carboxylated graphene and 12g of polyacrylic acid @ Co @ under continuous stirring40Fe40B20Respectively ultrasonically dispersing the powder for 20min, heating to 80 ℃ for reaction for 3.5h, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust the pH to 8, and filtering to respectively obtain the graphene-compounded acrylate adhesive and Co-compounded acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20The acrylate adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp once, 4 layers are coated, and finally the light release film is attached to the top layer to obtain the electromagnetic wave radiation resistant optical adhesive.
Example 3
An electromagnetic wave radiation preventing optical cement and a preparation method thereof, comprising the following steps:
(1) adding 0.6g of graphene oxide into 50ml of deionized water, carrying out ultrasonic treatment for 2h, uniformly dispersing to obtain a suspension, and adding 5g of NaOH and 10g of ClCH under continuous stirring2After the COOH is added dropwise, carrying out ultrasonic treatment for 4 hours, carrying out dialysis treatment on the mixture for 47 hours, then carrying out hot filtration on the dispersion liquid by using filter paper, collecting filtrate after a large number of graphene sheets pass through the filter paper, evaporating the solvent by using a rotary evaporator, and drying in an oven at 60 ℃ for 16 hours to obtain carboxylated graphene;
(2) 1.2g of boron block, 39.5g of FeCl2·4H2O and 47.5gCoCl2·6H2Dissolving O in 100ml of deionized water, adding 23g of polyacrylic acid into the solution, adding 10g of 0.1M sodium hydroxide solution, stirring uniformly to form a black solution, growing at 80 ℃ for 30min, and drying in a vacuum oven at 50 ℃ for 24h to obtain a product of @ polyacrylic acid Co40Fe40B20Powder;
(3) dissolving 2g of emulsifier SE-10 in 12ml of deionized water, transferring the solution to a constant temperature reactor, heating the solution to 80 ℃ and continuously stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving 82g of hydroxyethyl acrylate in 55ml of deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, stirring for 15min, and pre-emulsifying to obtain an emulsion;
(4) adding 20% of 85g of emulsion into a reactor, adding another 1 part of SE-10 solution of emulsifier, stirring uniformly, adding 1.5g of ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain a seed emulsion, dividing the seed emulsion into two parts, dividing the rest of emulsion into two parts, respectively adding the two parts into the seed emulsion, and respectively adding 4.8g of carboxylated graphene and 15g of polyacrylic acid Co @ under continuous stirring40Fe40B20Respectively ultrasonically dispersing the powder for 20min, heating to 80 ℃ for reaction for 4h, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust the pH to 7.5, and filtering to respectively obtain the graphene-compounded acrylate adhesive and Co-compounded acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20And 5 layers of acrylate adhesive are coated, the acrylic adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp every time, and finally the light release film is attached to the top layer to obtain the electromagnetic wave radiation prevention optical adhesive.
Example 4
An electromagnetic wave radiation preventing optical cement and a preparation method thereof, comprising the following steps:
(1) adding 0.6g of graphene oxide into 50ml of deionized water, carrying out ultrasonic treatment for 2h, uniformly dispersing to obtain a suspension, and adding 5g of NaOH and 11g of ClCH under continuous stirring2After the COOH is added dropwise, carrying out ultrasonic treatment for 3.8h, carrying out dialysis treatment on the mixture for 48h, then carrying out hot filtration on the dispersion liquid by using filter paper, allowing a large number of graphene sheets to pass through the filter paper, collecting filtrate, evaporating the solvent by using a rotary evaporator, and drying in an oven at 60 ℃ for 18h to obtain carboxylated graphene;
(2) 1.2g of boron block, 40g of FeCl2·4H2O and 47.5gCoCl2·6H2Dissolving O in 100ml deionized water, adding 25g of polyacrylic acid into the solution, adding 10g of 0.1M sodium hydroxide solution, stirring uniformly to form a black solution, growing at 80 ℃ for 30min, and drying in a vacuum oven at 50 ℃ for 24h to obtain a product of @ polyacrylic acid Co40Fe40B20Powder;
(3) dissolving 3g of emulsifier SE-10 in 15ml of deionized water, transferring the solution to a constant temperature reactor, heating the solution to 80 ℃ and continuously stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving 85g of hydroxyethyl acrylate in 60ml of deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, stirring for 15min, and pre-emulsifying to obtain an emulsion;
(4) adding 20% of 86g of emulsion into a reactor, adding 1 part of SE-10 solution of the emulsifier, stirring, adding 2g of ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain seed emulsion, dividing the seed emulsion into two parts, and emulsifying the restThe solution is divided into two parts, which are respectively added into the seed emulsion, and 5g of carboxylated graphene and 15g of polyacrylic acid @ Co are respectively added under continuous stirring40Fe40B20Respectively ultrasonically dispersing the powder for 20min, heating to 80 ℃ for reaction for 4h, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust the pH to 8, and filtering to respectively obtain the graphene-compounded acrylate adhesive and Co-compounded acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20And 5 layers of acrylic adhesive are coated, the acrylic adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp each time, and finally the light release film is attached to the top layer to obtain the electromagnetic wave radiation prevention optical adhesive.
Comparative example 1
An optical cement and a preparation method thereof comprise the following steps:
(1) dissolving 1g of emulsifier SE-10 in 10ml of deionized water, transferring the solution to a constant temperature reactor, heating the solution to 80 ℃ and continuously stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving 75g of hydroxyethyl acrylate in 50ml of deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, stirring for 15min, and pre-emulsifying to obtain an emulsion;
(2) adding 20% of 80g of emulsion into a reactor, adding another 1 part of SE-10 solution of the emulsifier, stirring uniformly, adding 1g of ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain seed emulsion, dividing the seed emulsion into two parts, dividing the rest of the emulsion into two parts, respectively adding the seed emulsion into the seed emulsion, and respectively adding 0.5g of graphene and 2g of Co under continuous stirring40Fe40B20Respectively ultrasonically dispersing for 20min, heating to 80 ℃ for reaction for 3.5h, cooling to 60 ℃, dropwise adding dimethylethanolamine to adjust the pH to 7, and filtering to respectively obtain the graphene-doped acrylate adhesive and Co-doped acrylate adhesive40Fe40B20Acrylate adhesives of (1);
(3) sequentially coating and compounding on heavy release filmGraphene-doped acrylate adhesives and Co-doped acrylates40Fe40B20The acrylate adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp once, the coating is carried out for 2 times in total, and finally the light release film is attached to the top layer to obtain the optical adhesive.
Comparative example 2
The difference from example 4 is that ethyl acrylate is used as a monomer instead of hydroxyethyl acrylate, and is coated only twice in step (5), resulting in an optical adhesive for preventing electromagnetic wave radiation.
And (3) testing:
1) electromagnetic shielding performance test:
the electromagnetic shielding performance of the films was tested using a ME7838A vector network analyzer, and examples 1-5 and comparative examples 1-2 were cut into 22.9mm long by 10.2mm wide test samples at a test frequency of 8.2-12.8GHz, as shown in Table 1.
Table 1:
2) mechanical property test:
tensile strength and elongation at break of the optical cement were measured using an optical instrument using the cement tensile strength test method, examples 1-5 and comparative examples 1-2 were cut into 25mmx25mm test specimens, a universal tester was loaded at a rate of 2mm/min until the specimens were broken, and the tensile strength and elongation at break of the test specimens were recorded and the results are shown in table 2.
Table 2:
in summary, it can be seen from tables 1 and 2 that the tensile strength and elongation at break of the optical adhesives for shielding electromagnetic radiation prepared in examples 1-4 tend to increase with the number of film layers, and the reflection loss capability and shielding effect thereof gradually increase with the number of film layersEnhanced, whereas comparative example 1 did not target nanoparticle graphene and Co40Fe40B20The modified nano-particles are directly doped into the acrylate adhesive, the nano-particles are not uniformly dispersed and are only coated twice, so that the shielding effect is low, the ethyl acrylate is used for replacing hydroxyethyl acrylate in the comparative example 2, and the carboxylated graphene and Co are40Fe40B20The reaction with ethyl acrylate is not carried out, which also shows that the carboxyl on polyacrylic acid and Co are utilized to carry out carboxylation on graphene oxide40Fe40B20The coordination is carried out and then the coordination is grafted to the polyhydroxyethyl acrylate, so that the stability and the mechanical property of the nano particles and the acrylate adhesive are improved, and Co is compounded40Fe40B20After the acrylate adhesive and the acrylate adhesive compounded with the graphene are alternately paved and coated in multiple layers, an absorption-reflection-reabsorption process can be formed in the acrylate adhesive, so that an efficient electromagnetic radiation effect is realized.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation method of an anti-electromagnetic wave radiation optical cement is characterized by comprising the following steps:
(1) adding graphene oxide into deionized water, carrying out ultrasonic treatment for 2h, dispersing uniformly to obtain a suspension, and adding NaOH and ClCH under continuous stirring2Performing ultrasonic treatment after the COOH is added dropwise, performing water dialysis treatment on the mixture, performing hot filtration on the dispersion liquid by using filter paper, allowing a large number of graphene sheets to pass through the filter paper, collecting the filtrate, evaporating the solvent by using a rotary evaporator, and drying to obtain carboxylated graphene;
(2) mixing boron block and FeCl2·4H2O and CoCl2·6H2Dissolving O in deionized water, adding polyacrylic acid into the solution, adding precipitant, stirring to obtain black solution, growing at 80 deg.C for 30min, and drying to obtain polyacrylic acid @ Co40Fe40B20Powder;
(3) dissolving an emulsifier SE-10 in deionized water, transferring the deionized water into a constant temperature reactor, heating the deionized water to 80 ℃ under continuous stirring to obtain an emulsifier SE-10 solution, uniformly dividing the emulsifier SE-10 solution into 2 parts, dissolving hydroxyethyl acrylate in the deionized water at 80 ℃ to obtain a solution A, adding 1 part of the emulsifier SE-10 solution into the solution A, and stirring for 15min for pre-emulsification to obtain an emulsion;
(4) adding 20% of the emulsion into a reactor, adding another 1 part of SE-10 solution of the emulsifier, stirring uniformly, adding ammonium persulfate, heating to 80 ℃, stirring for 30min to obtain a seed emulsion, dividing the seed emulsion into two parts, dividing the rest of the emulsion into two parts, respectively adding the seed emulsion into the seed emulsion, and respectively adding the carboxylated graphene and the polyacrylic acid @ Co under continuous stirring40Fe40B20Respectively carrying out ultrasonic treatment reaction on the powder, cooling to 60 ℃, then dropwise adding dimethylethanolamine to adjust to a target pH value, and filtering to respectively obtain the graphene-compounded acrylate adhesive and the Co40Fe40B 20-compounded acrylate adhesive;
(5) the heavy release film is sequentially coated with the acrylate adhesive compounded with graphene and the Co40Fe40B20The acrylate adhesive is coated for the next time after being sequentially cured by a mercury lamp and a metal halogen lamp every time, and the coating is 3And (5) finally, attaching the light release film to the top layer to obtain the electromagnetic wave radiation resistant optical adhesive.
2. The method for preparing an optical adhesive for preventing electromagnetic wave radiation according to claim 1, wherein the particle size of the graphene oxide in the step (1) is 10-50 nm.
3. The method for preparing an electromagnetic radiation shielding optical cement according to claim 1, wherein the graphene oxide, NaOH and ClCH in step (1)2The mass ratio of COOH is 0.4-0.6:5:9-11, and NaOH and ClCH are dropwise added in the step (1)2The ultrasonic treatment time after COOH is 3-4h, the water dialysis treatment time is 45-48h, and the drying condition is drying in an oven at 60 ℃ for 12-18 h.
4. The method for preparing an electromagnetic radiation shielding optical cement according to claim 1, wherein in the step (2), polyacrylic acid, boron block, FeCl2·4H2O、CoCl2·6H2The mass ratio of O to deionized water is 18-25:1-1.2:39-40:47-47.5:100, and the precipitator in the step (2) is 0.1M sodium hydroxide solution, and the amount of the precipitator is 1/10 of deionized water.
5. The method for preparing an optical adhesive for preventing electromagnetic wave radiation according to claim 1, wherein the drying condition in the step (2) is drying in a vacuum oven at 50 ℃ for 24 hours.
6. The method for preparing the electromagnetic wave radiation preventing optical cement as claimed in claim 1, wherein the mass ratio of the emulsifier SE-10 to the hydroxyethyl acrylate in the step (3) is 1-3:75-85, the mass ratio of the emulsifier SE-10 to the deionized water is 1-3:10-15, and the mass ratio of the hydroxyethyl acrylate to the deionized water is 75-85: 50-60.
7. The method for preparing an optical adhesive for preventing electromagnetic wave radiation according to claim 1The method is characterized in that in the step (4), the carboxylated graphene, the polyacrylic acid @ Co40Fe40B20The mass ratio of the powder to the emulsion to the ammonium persulfate is 4-5:10-15:80-86: 1-2.
8. The method for preparing an optical adhesive for preventing electromagnetic radiation according to claim 1, wherein the reaction conditions of the ultrasonic treatment in the step (4) are ultrasonic dispersion for 20min, heating to 80 ℃ and reaction for 3-4h, and the target pH is 7-8.
9. An electromagnetic radiation shielding optical adhesive prepared by the preparation method of any one of claims 1 to 8.
10. The optical cement for preventing electromagnetic wave radiation as claimed in claim 9, wherein the heavy release film and the light release film are both ultra-light fluorine release films, the release force of the heavy release film is 25-35g, and the release force of the light release film is 8-14 g.
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